Process of manufacturing smokeless powder.



No. 837,463. PATENTED DEC. 4, 1906. G. W. GENTIEU. PROCESS OF MANUFACTURING SMOKELESS POWDER.

APPLICATION FILED APR. 2. 1906.

INVENTOR UNITED sTApEs PATENT OFFICE.

GEORGE V. GENTIEU, OF PEORIA, ILLINOIS.

PROCESS OF MANUFACTURING SMOKELESS POWDER.

Specification of Letters Patent.

Patented Dec. 4, 1906.

Application filed April2,1906. Serial No. 309,485.

oria, m the county of Peoria and State of Illinois, have invented'cer'tain new and useful Improvements in Processes of Manufacturing Smokeless Powder; and I do hereby declare the following to be a. full, clear,- and exact description of the invention, such as will enable others skilled in the art to which it appcrtains to make and use the same.

My invention consists in the novel features hereinafter described, reference being had to the accompanying drawings, whichillustrate one form of apparatus for carrying my proccess into effect; and my invention is fully disclosed in the followingdcsc-ription and claims.

Referring to the said drawings, Figure 1 represents a sectional view, partly in elevation. of an improved apparatus which I prefer to employ in carrying my process into effect, although I do not confine myself to the st ylc of apparatus shown, as other apparatus may be used in which the same principle involved by my process could be employed. Fig. 2 is a detail sectional view of the spraying device and valve. Figs. 3 and 4 are detail views of the spraying-nozzle.

My invention relates to improvements in the manufacture of explosive compounds, especially to that class known as smokeless gunpowders and which are made from nitrated cellulose, or guncotton.

It consists in an improved process whereby finely-divided or pulped nitrocellulose containing from fifteen per cent. to forty per cent. of water is agitated in a suitable receptacle, and during such agitation while the. moist nitrocellulose is being hurled upward from the bottom of the receptacle it is brought 1 finely-ground nitrocellulose, after 1t has been into violent contact with a descending stream of solvent which is soluble in water. This solvent is delivered at a constant degree of pressure, approximately one hundred and twenty-five pounds per square inch, and by means of the velocity imparted to the streams by this pressure is driven into the particles of moist nitrocellulose and, combining with the water, effects a slowcolloid= ing of the nitrocellulose, aft-er which the colloided or gelatinized particles are removed to any form of well-known solventrecovery apparatus (not shown) and the solvent recovered.

y the powder be less liable to The main objects of m invention are to produce a gunpowder w iich shall have a greater stability than is possible by the use of other methods, to overcome all danger to workmen and apparatus by using moist nitrocellulose, to produce a powder-grain more compact and less porousin ordcri'that' absorb inoisture from the atmosphere.

Another object is to use solvents miscible in water and having a lower boiling-point than water in order that the solvent and water may be removed from the powder-grains with a lower degree of heat than would be necessary to use with solvents of high boiling-point.

These objects and manner of reaching same are more clearly hereinafter set forth.

My process enables me to produce a powder that does not deteriorate with age, is practically unaffected by changes of atmospheric conditions due to the compact nature of the grain, and owing to the simple and inexpensive machinery re uired it can be produced at a less cost than y anyother process now known. The valuable Solvents can also be recovered easily without injury to the powder. Owing to the volatile nature of the solvents, a low degree of heat (43 centigrade) is required. By the use of my process the danger to workmen is entirely removed, as the powder is made in the wet stage and is practically unexplosive.

in carrying my improved process into effect I take nitrocellulose of the suit-able degree of nitration to make the desired smokeless powders. For example, for making powders adapted for use in shot-guns and rifles I grind, pulp, or beat the nitrocellulose into a finer state than is usually the case, the reason for which will be hereinafter explained. This thoroughly cleansed from acid and has passed the necessary heat or stability tests equal to the requirements of the United States Governmcnt, is treated in a centrifugal wringer, operated at very high speed, until the quantity of water left in the nitrocellulose is from fifteen per cent. to forty per cent., the quantity of water left in the nitrocellulose par tially determining the density of the grain of the finished powder. The nitrocellulose is now introduced into a suitable vessel fitted with an agitating or stirring device provided with swiftly-revolving blades and is rapidly I agitated. The nitrocellose while being thrown miscible in water, which is discharged with considerable force into the vessel and coming with great speed in contact with the damp nitrocellulose is driven into the mass or particles, breaking the nitrocellulose into smaller aims, at the same time permeating into the interior of the grains, combining with the water, and forming a deterrent solvent, which colloids the grains to the required degree necessary to produce a stable powder.

The size of the grains and the quantity of a marketable roduct is influenced to a marked'extent by the degree of fineness to which the nitrocellulose is ground, pulped, or beaten. This is due to the tendency of the cellulose materials to mat or collect together in large lumps. The size and quantity of grain is also regulated in part by the speed of the stirrer-shaft and the force with which the descending spray. of solvent strikes the nitrocellulose, also the per cent. of moisture left in the nitrocellulose. By carefully regulating the different operations Iam enabled to produce satisfactory results.

The solvents I prefer to use are the well known solvents ethyl and methyl alcohol,

acetone, or'any other suitable solvent whose great extent in water.

boiling or evaporating point is below that of.

water and which are miscible or soluble to a By driving the solvent into the wet-nitrocellulose grains, as before described, the solvent and water in the grains immediately combine, forming a deterrent solvent, which immediately acts uniformly u on all ortions of the grains, colloiding t em to t e desired degree.

Owing to the fact that water when mixed with a larger proportion of a solvent miscible with it of alower boiling-point boils at nearly the same degree of heat as the liquid of the lowest boiling-point, I am enabled to successfully remove the solvent and water by the use of a low degree of heat, thus producing a powder whose stability has not been injured to theleast extent by use of excessive heat,

and I also recover the valuable solvent. The

' amount of steam or heat saved is an important factor in the cost of production.

*' It is of the utmost importance that the I lowest possible degreeof heat be employed in the manufacture of the powder and removal of the solvent in order to maintain the sta- .cess. of 140 Fahrenheit, the higher the temperature the quicker the rate of decomposition. For example, the best purified nitrocellulose will begin to decompose in twenty to eighty minutes at 150 Fahrenheit, while at 212 Fahrenheit (the boiling-point of water) decomposition -takes place in less than ten minutes, and at 365 Fahrenheit the best nitrocellulose will explode. At temperatures of 120 Fahrenheit and lower nitrocellulose is very stable and will stand without any trace of decomposition for months and years, so that powder manufactured at a low degree of heat will be able to stand for years Without any chemical change taking place. I do not employ a higher degree of heat than 110 Fahrenheit to remove the solvent, while the powder is manufactured at ordinary atmospheric temperatures, no artificial heat being used. I am thus enabled to maintain the original stability of the nitrocellulose unimpaired.

In order that my improved process may be more clearly understood, I have illustrated in the accompanying drawings an apparatus which I prefer to employ for carrying the process into effect.

. In the drawings, A represents a receptacle or tank, preferably cylindrical in form, sup ported in any desired manner and provided with manholes at top and bottom clos'edby manhole-covers G and G for the introduction and removal of the nitrocellulose. A stirrer shaft or axle B passes through the cylindrical tank A, is mounted in suitable bearings, and provided with driving means, such aspulleys b, as shown, for driving it at various speeds. Vithin the tank A the shaft B is provided with a series of radial agitat ng arms or blades C for the purpose of tossing the nitrocellulose upward and thoroughly agitating'it. The arms or blades are preferably arranged in positions at equaldistances around the shaft or axle B.

J represents a small cylindrical tank which is used as a receptacle or reservoir to c-ontam the solvent.

f is the suction-pipe connecting the reservoir J with the small steam-pump F and 1s provided with the controlling gate-valve g in order to shut off the supply of solvent when desired.

f is the delivery or discharge pipe which delivers the solvent from the pump F to the jet-valves D D D.

H is an angle-lever safety-valve provided with an adjustable weight and which is set to open at a certain pressure to deliver the surplus solvent through the pipe h back to the reservoir J.

D represents a three-way jet-valve provided with needle-valve d and a fan-shaped manifold spraying-nozzle E, through which the solvent is delivered at a'high pressure with great velocity into the nitrocellulose.

In using this apparatus to carry my improved process into' effect the pulped nitrocellulose having been treated in a centrifugal Wringer until only the desired percentage of the shaft or axle B is revolved at the desired a speed, and the moist nitrocelluloseis agitated and thrown upward by means of the arms or blades C. The desired solvent, which is V miscible in water,'has previously been introduced in the reservoir J, "and the pum F being set in motion draws the solvent t ough the suction-pipe f the valve 9 being open, and delivers it under ressure through the pipeto the j et-valves D D and thence discharges it through the fan-shaped manifold.

spraying-nozzles E E E in fine streams. of very high velocity, and coming into contact with the mass or grains of moist nitrocellulose the solvent is driven into the material with great force, breaking it into smaller particles or grains, at the same time combining with the water in the nitrocellulose to effect a deterrent colloiding of the nitrocellulose, thus enabling the grams to become coll-oided slowly and uniformly throughout the entire mass.

In order to obtain the high ressure at a uniform rate, I use a pump F o agreater delivering ca acity than the jet-valves D D D and provi e the safety-valve H on the deliveryipef to deliver the surplus solvent back to t e reservoir J through the overflow-pipe 'h. The safety-valve H will ordinarily be set to openat about one hundred and twentyfive pounds to the square inch;-but I do not limit myself to the exact ressure. The desired quantity of solvent aving been injected into the moist nitrocellulose and suffi- .cient time (usually two tofour hours) having been allowed in which to colloid the grains to the desired degree, the wet grains are now removed through the lower manhole G' and placed in any suitable solvent-recovery apparatus, (not shown,) in which the powder is exposed to a tem erature not exceedin 43 centigrade, andt e powder is thus drie and the solvent recovered at leisure. The rains are then sieved and will form a va uable smokeless owder.

To aid t e combustion of the nitrocellulose, limited quantities of nitrate of potasslum, nitrate of barium, nitrate of sodium, or

7' other nitrates possessing the requisite peris not facturing explosives which consists in agitating finely-dlvided nitrocellulose, contalning water to the extent of not less than fifteen per cent. and not exceeding forty er cent.,

and injecting into it at a pressure 0 substantially one hundred and twenty-five pounds per s uare inch, during such agitation, a solvent aving a boiling-point lower than that of water, to drive the solvent into the particles of nitrocellulose, and cause it to unite with the watertherein, to produce a diluted solvent of lower boilin -point than water, and to effect a deterrent co loiding of the nitrocellulose grains, then subjecting the colloided grains to heat at a temperature not exceeding 43 centigrade to recover the surplus solvent and dry the grains. g

2. The herein-described process of manu facturin explosives which consists in agitating fine y-divided nitrocellulose contain ng water in excess of fifteen per cent, mjectm into the material during such a itation a so vent soluble in and having a ower boilingpoint than water, to cause the solvent to unite with the water in the nitrocellulose, and

uniformly and slowly colloid the grains thereof, then treating the colloided grains with heat at lower temperature than the boiling-point of water to recover the surplus I solvent, and dry' the grains.

3. The herein-described process of-manufacturin explosives, which consists in agitating fine y-dlvided nitrocellulose containing water in excess of fifteen er cent. and treating it with a solvent, solu le in and havin a lower boiling-point than water, to cause t e solvent to unite with the water in the'nitrocellulose, and uniformly colloid the grains,

and then drying the grains. 1 In testimony whereof I affix my in the presence of two witnesses.

signature GEORGE W. GENTIEU. Witnesses:

MARY E. OOMEGYS,'

E. M. Guns. 

